CN104880449B - A kind of ammonia nitrogen fluorescence detection method - Google Patents
A kind of ammonia nitrogen fluorescence detection method Download PDFInfo
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- CN104880449B CN104880449B CN201510335921.8A CN201510335921A CN104880449B CN 104880449 B CN104880449 B CN 104880449B CN 201510335921 A CN201510335921 A CN 201510335921A CN 104880449 B CN104880449 B CN 104880449B
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Abstract
The invention discloses a kind of ammonia nitrogen fluorescence detection method, including ammonia nitrogen fluorescence detection device, described device includes ammonia generation bottle, reaction film frame and detection bottle, and the ammonia generation bottle is wide-mouth bottle；The reaction film frame includes the mounting table and hanger bracket that middle part is through hole, and the mounting table and hanger bracket are connected as a single entity；The detection bottle is fitted with ultra violet light emitter, and the side for detecting bottle is provided with transparent observing window；The bottleneck of ammonia generation bottle connects with detecting the bottom of bottle, and reaction film frame is set in junction of the ammonia generation bottle with detecting bottle.This device is convenient for carrying, and operation is simple, and layman is operable, is adapted to wide；This method only need to be by eye observation reaction film shade compared with standard color comparison card, you can judges the concentration of ammonia nitrogen in water sample, water sample is without filtering, and simplicity is quick, the degree of accuracy is higher.
Description
Technical field
The present invention relates to water body ammonia nitrogen detection field, especially a kind of ammonia nitrogen fluorescence detection method.
Background technology
Ammonia nitrogen is the nutriment of algae substances, can make water body that eutrophication occur, so that water hypoxia, water quality
Deteriorate, the aquatile such as fish can not survive.It is sub- meanwhile under aerobic conditions, ammonia nitrogen can be nitrite nitrogen by microbiological oxidation
Nitrate nitrogen is combined generation nitrosamine with protein, has carcinogenic and teratogenesis.Therefore, ammonia nitrogen concentration can reflect water in water body
The contaminated degree of body, it is that surface water quality and fishery water water quality must survey one of index.
The ammonia nitrogen detection method reported has gassensing ammonia electrode method, visible spectrophotometry and fluorescent spectrometry etc., these
Method needs instrument and equipment and the professional person's operation of specialty, it is difficult to towards layman such as fishermen.
The content of the invention
It is an object of the invention to provide a kind of ammonia nitrogen fluorescence detection device and detection method, this device is convenient for carrying, behaviour
Make simply, layman is operable, is adapted to wide；This method need to only pass through eye observation reaction film shade and mark
Quasi- colorimetric card compares, you can judges the concentration of ammonia nitrogen in water sample, simplicity is quick, the degree of accuracy is higher.
Realizing the technical scheme of the object of the invention is：
A kind of ammonia nitrogen fluorescence detection device, including
Ammonia generates bottle, and for being ammonia by the mineralized nitrogen in water sample, the ammonia generation bottle is wide-mouth bottle；
Reaction film frame, for placing response film, the reaction film frame includes the mounting table and hanger bracket that middle part is through hole, institute
State mounting table and hanger bracket is connected as a single entity；
Bottle, the shade of the fluorescence sent for observing response film are detected, the detection bottle is fitted with ultraviolet light emission
Device, the side of the detection bottle are provided with transparent observing window；
The bottleneck of the ammonia generation bottle connects with detecting the bottom of bottle, and reaction film frame is set in ammonia generation bottle and detection
The junction of bottle.
The mounting table and hanger bracket are screwed by screw thread, are spirally connected and are connected as a single entity.
The bottleneck band external screw thread of ammonia generation bottle, detection bottle carry the internal thread being adapted to ammonia generation bottle, the ammonia
The bottleneck for generating bottle is connected through a screw thread with detecting the bottom of bottle.
Ammonia nitrogen in water sample includes NH4 +And NH3Two kinds of forms.
Using the ammonia nitrogen fluorescence detection method of said apparatus, comprise the following steps：
1）Take 50 mL water samples to be placed in ammonia generation bottle from sample source, add 5mL cushioning liquid；
2）Take a reaction film to be placed on the mounting table of reaction film frame, detection bottle is screwed with ammonia generation bottle and is connected, is examined
Bottle is surveyed to be disposed vertically upper；
3）Gently yawing detection means, mix step 1）Reaction solution, stand 2-3 hours, make ammonia abundant with reaction film
Reaction；
4）Ultra violet light emitter is opened, from the color of watch window observing response film, reference standard colorimetric card, standard colorimetric
Concentration corresponding with the immediate color of the reaction film is the ammonia nitrogen concentration value of the water sample in card；
The preparation of the cushioning liquid：Reagent bag 1 is dissolved in 50 mL pure water and is formulated；The reagent bag 1 is
2.6 g disodium ethylene diamine tetraacetates（EDTA）Mixed with 1.0 g NaOH solids；
The preparation of the reaction film includes：
a）Reaction film soak：Reagent bag 2 is dissolved in 50 mL pure water, is configured to reaction film soak；The reagent
Bag 2 is 0.03975g OPA（OPA）With 0.0125g Na2SO3Solid mixes；
b）React film production：Quantitative filter paper is cut into the mm of diameter 32 circular small filter paper, is placed in reaction film soak
15 min-120 min are soaked, filter paper is fully absorbed reaction reagent OPA and Na in soak2SO3；
The preparation of the standard color comparison card includes：
A each 50 mL of serial Ammonia nitrogen standard liquid in the range of 2-32 μm of ol/L) is prepared, pours into detection means respectively
In ammonia generation bottle, 5 mL cushioning liquid are added；
B）Take a reaction film to be placed on the mounting table of reaction film frame, detection bottle is screwed with ammonia generation bottle and is connected, is examined
Bottle is surveyed to be disposed vertically upper；
C）Gently yawing detection means, mix step A）Reaction solution, stand 2-3 hours, make ammonia abundant with reaction film
Reaction；
D）Unlatching ultra violet light emitter, the color of the reaction film of the standard liquid of various concentrations from watch window, and
The color color lump of the reaction film of the standard liquid for each various concentrations observed is drawn out in control, and these then are represented into difference
The standard color block of concentration is printed on colorimetric card carrier, and carrying out corresponding concentration value to each standard color block marks.
Judge the concentration of water sample：Ultra violet light emitter is opened, from the color of watch window observing response film, reference standard ratio
Colour atla, concentration corresponding with the immediate color of the reaction film is the concentration of the water sample in standard color comparison card, if reaction film
Color can therebetween be estimated between the concentration of standard color comparison card two and read a concentration.
The principle of the present invention：It is NH by the mineralized nitrogen in water sample3, and immersed with OPA（OPA）And Na2SO3Examination
The filter paper of agent is that solid phase fluorescent reaction occurs for reaction film, under the irradiation of uviol lamp, the fluorescence color depth that reaction film is sent with
Ammonia nitrogen concentration is relevant in water sample.
This device is convenient for carrying, and operation is simple, and layman is operable, is adapted to wide；This method need to only lead to
Eye observation reaction film shade is crossed compared with standard color comparison card, you can judge the concentration of ammonia nitrogen in water sample, water sample without
Need to filter, simplicity is quick, the degree of accuracy is higher.
Brief description of the drawings
Fig. 1 is the structural representation of ammonia nitrogen fluorescence detection device in embodiment；
Fig. 2 is the structural representation of reaction film frame in embodiment；
Fig. 3 is embodiment Plays colorimetric card schematic diagram.
In figure, the hanger bracket 4. of 1. ammonias generation bottle, 2. mounting table 3. detects the observation window of 5. ultra violet light emitter of bottle 6.
7. through holes of mouth.
Embodiment
Present invention is further elaborated with reference to the accompanying drawings and examples, but is not limitation of the invention.
Embodiment：
The Fig. 2 of reference picture 1, a kind of ammonia nitrogen fluorescence detection device, including
Ammonia generates bottle 1, and for being ammonia by the mineralized nitrogen in water sample, the ammonia generation bottle 1 is wide-mouth bottle；
Reaction film frame, for placing immersed with OPA and Na2SO3The filter paper of reagent is reaction film, the reaction film
Frame includes the mounting table 2 and hanger bracket 3 that middle part is through hole 7, and the mounting table 2 and hanger bracket 3 are connected as a single entity；
Bottle 4, the shade of the fluorescence sent for observing response film are detected, the detection bottle 4 is fitted with ultraviolet light hair
Emitter 5, the side of the detection bottle 4 are provided with transparent observing window 6；
The bottleneck of ammonia generation bottle 1 connect with the bottom of detection bottle 4, reaction film frame be set in ammonia generate bottle 1 and
Detect the junction of bottle 4.
The mounting table 2 and hanger bracket 3 are screwed by screw thread, are spirally connected and are connected as a single entity.
The bottleneck band external screw thread of ammonia generation bottle 1, detection bottle 4 carry the internal thread being adapted to ammonia generation bottle 1, the ammonia
The bottleneck of gas generation bottle 1 is connected through a screw thread with detecting the bottom of bottle 4.
Using the ammonia nitrogen fluorescence detection method of said apparatus, comprise the following steps：
1）Take 50 mL water samples to be placed in ammonia generation bottle 1 from sample source, add 5mL cushioning liquid；
2）Take a reaction film to be placed on the mounting table 2 of reaction film frame, detection bottle 4 screwed with ammonia generation bottle 1 and is connected,
Detection bottle 4 is disposed vertically upper；
3）Gently yawing detection means, mix step 1）Reaction solution, stand 2-3 hours, make ammonia abundant with reaction film
Reaction；
4）Ultra violet light emitter 5 is opened, from the color of the observing response film of watch window 6, reference standard colorimetric card, standard ratio
Concentration corresponding with the immediate color of the reaction film is the ammonia nitrogen concentration value of the water sample in colour atla；
The preparation of the cushioning liquid：Reagent bag 1 is dissolved in 50 mL pure water and is formulated；The reagent bag 1 is
2.6 g disodium ethylene diamine tetraacetates（EDTA）Mixed with 1.0 g NaOH solids；
The preparation of the reaction film includes：
a）Reaction film soak：Reagent bag 2 is dissolved in 50 mL pure water, is configured to reaction film soak；The reagent
Bag 2 is 0.03975g OPA（OPA）With 0.0125g Na2SO3Solid mixes；
b）React film production：Quantitative filter paper is cut into the mm of diameter 32 circular small filter paper, is placed in reaction film soak
15 min-120 min are soaked, filter paper is fully absorbed reaction reagent OPA and Na in soak2SO3；
The preparation of the standard color comparison card includes：
A each 50 mL of serial Ammonia nitrogen standard liquid in the range of 2-32 μm of ol/L) is prepared, pours into detection means respectively
In ammonia generation bottle, 5 mL cushioning liquid are added；
B）Take a reaction film to be placed on the mounting table 2 of reaction film frame, detection bottle 4 screwed with ammonia generation bottle 1 and is connected,
Detection bottle 4 is disposed vertically upper；
C）Gently yawing detection means, mix step A）Reaction solution, stand 2-3 hours, make ammonia abundant with reaction film
Reaction；
D）Unlatching ultra violet light emitter 5, the color of the reaction film of the standard liquid of various concentrations from watch window 6,
And the color color lump of the reaction film for the standard liquid for drawing out each various concentrations observed is compareed, then by these representatives not
Standard color block with concentration is printed on colorimetric card carrier, and carrying out corresponding concentration value to each standard color block marks.It is different
Standard color comparison card color is as shown in Figure 3 corresponding to ammonia nitrogen concentration.
Specifically, determined using this detection means and method and pick up from Guilin City Lingchuan County Hua Jiang Guilin Electronic Science and Technology Univ.
Section it is upper, in, each 3 water samples in downstream, the sampling time is on May 7th, 2015, respectively with this detection means and method, and
Indophenol blue spectrophotometric method determines, each parallel determination 3 times, as a result as shown in table 1.
The water determination result of table 1
As can be seen from Table 1, it is very close with indophenol blue method to measure result for the present apparatus and concentration measured by method, poor
It is different within 10%, it is seen that the present apparatus and method can be compared with the concentration of ammonia nitrogen in Accurate Determining water body, compared to indophenol blue method, this
Device is simple to operate, as a result accurately, is convenient for carrying, and water sample is without filtering, and layman is operable.
Claims (1)
- A kind of 1. ammonia nitrogen fluorescence detection method, it is characterised in that including ammonia nitrogen fluorescence detection device, the ammonia nitrogen fluoroscopic examination dress Put includingAmmonia generates bottle, and for being ammonia by the mineralized nitrogen in water sample, the ammonia generation bottle is wide-mouth bottle；Reaction film frame, for placing response film, the reaction film frame includes the mounting table and hanger bracket that middle part is through hole, described to put Put platform and hanger bracket is connected as a single entity；Bottle, the shade of the fluorescence sent for observing response film are detected, the detection bottle is fitted with ultra violet light emitter, institute The side for stating detection bottle is provided with transparent observing window；The bottleneck of the ammonia generation bottle connects with detecting the bottom of bottle, and reaction film frame is set in ammonia generation bottle with detecting bottle Junction；The ammonia nitrogen fluorescence detection method comprises the following steps：1）Take 50 mL water samples to be placed in ammonia generation bottle from sample source, add 5mL cushioning liquid；2）Take a reaction film to be placed on reaction film frame, detection bottle is screwed with ammonia generation bottle and is connected, detection bottle is upper vertical Place；3）Gently yawing detection means, the reaction solution of step 1 is mixed, stand 2-3 hours, ammonia is fully reacted with reaction film；4）Ultra violet light emitter is opened, from the color of watch window observing response film, reference standard colorimetric card, in standard color comparison card Concentration corresponding with the immediate color of the reaction film is the ammonia nitrogen concentration value of the water sample；The preparation of the cushioning liquid：Reagent bag 1 is dissolved in 50 mL pure water and is formulated；The reagent bag 1 is 2.6 g Disodium ethylene diamine tetraacetate and 1.0 g NaOH solids mix；The preparation of the reaction film includes：a）Reaction film soak：Reagent bag 2 is dissolved in 50 mL pure water, is configured to reaction film soak；The reagent bag 2 The Na of OPA and 0.0125g for 0.03975g2SO3Solid mixes；b）React film production：Quantitative filter paper is cut into the mm of diameter 32 circular small filter paper, is placed in the immersion of reaction film soak 15 min-120 min, filter paper is set to fully absorb reaction reagent OPA and Na in soak2SO3；The preparation of the standard color comparison card includes：A）Each 50 mL of serial Ammonia nitrogen standard liquid in the range of 2-32 μm of ol/L is prepared, pours into the ammonia life of detection means respectively Into in bottle, 5 mL cushioning liquid are added；B）Take a reaction film to be placed on the mounting table of reaction film frame, detection bottle is screwed with ammonia generation bottle and is connected, detects bottle It is disposed vertically upper；C）Gently yawing detection means, mix step A）Reaction solution, stand 2-3 hours, ammonia is fully reacted with reaction film；D）Ultra violet light emitter, the color of the reaction film of the standard liquid of various concentrations from watch window are opened, and is compareed The color color lump of the reaction film of the standard liquid for each various concentrations observed is drawn out, these are then represented into various concentrations Standard color block be printed on colorimetric card carrier, carrying out corresponding concentration value to each standard color block marks.
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105510325A (en) * | 2015-12-08 | 2016-04-20 | 浙江省嘉兴市农业科学研究院（所） | Semiquantitative determination method of concentration of ammonium nitrogen in agricultural biogas fluid |
| CN107091823A (en) * | 2016-02-18 | 2017-08-25 | 常州罗盘星检测科技有限公司 | A kind of low-concentration ammonia-nitrogen fluoroscopic examination solid reagent and its detection method |
| CN105866088B (en) * | 2016-05-20 | 2019-01-11 | 山东省科学院海洋仪器仪表研究所 | A kind of device and method of on-line checking Ammonia In Sea Water nitrogen content |
| CN110455767A (en) * | 2019-09-06 | 2019-11-15 | 四川轻化工大学 | Portable and visual blood ammonia rapid fluorescence detection device and its preparation and application |
| CN110596031A (en) * | 2019-10-14 | 2019-12-20 | 中国科学院烟台海岸带研究所 | Quantitative analysis device for ammonia nitrogen in seawater |
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| CN103018219A (en) * | 2012-12-07 | 2013-04-03 | 桂林电子科技大学 | Application of 4,5-dimethoxyphthalaldehyde in detection of ammonium nitrogen in water and determination method |
| CN104111245A (en) * | 2014-07-29 | 2014-10-22 | 桂林电子科技大学 | Method for reducing reagent blank in detection of ammonium nitrogen by use of o-phthalaldehyde fluorescence method |
| CN104515762A (en) * | 2015-01-19 | 2015-04-15 | 桂林电子科技大学 | Solid-phase fluorescence analysis method for determining ammonium nitrogen in water sample by taking filter paper as carrier |
| GB2519937A (en) * | 2013-09-05 | 2015-05-13 | Kanichi Res Services Ltd | Electrochemical sensor |
| CN204731161U (en) * | 2015-06-17 | 2015-10-28 | 桂林电子科技大学 | A kind of ammonia nitrogen fluorescence detection device |
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| CN103018219A (en) * | 2012-12-07 | 2013-04-03 | 桂林电子科技大学 | Application of 4,5-dimethoxyphthalaldehyde in detection of ammonium nitrogen in water and determination method |
| GB2519937A (en) * | 2013-09-05 | 2015-05-13 | Kanichi Res Services Ltd | Electrochemical sensor |
| CN104111245A (en) * | 2014-07-29 | 2014-10-22 | 桂林电子科技大学 | Method for reducing reagent blank in detection of ammonium nitrogen by use of o-phthalaldehyde fluorescence method |
| CN104515762A (en) * | 2015-01-19 | 2015-04-15 | 桂林电子科技大学 | Solid-phase fluorescence analysis method for determining ammonium nitrogen in water sample by taking filter paper as carrier |
| CN204731161U (en) * | 2015-06-17 | 2015-10-28 | 桂林电子科技大学 | A kind of ammonia nitrogen fluorescence detection device |
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Effective date of registration: 20200703 Address after: C413-5, floor 4, block a, information incubation building, No. D-12, information industry park, high tech Zone, Qixing District, Guilin City, Guangxi Zhuang Autonomous Region Patentee after: Guilin Derun Testing Co., Ltd Address before: 541004 the Guangxi Zhuang Autonomous Region golden Guilin Qixing District Road No. 1 Patentee before: GUILIN University OF ELECTRONIC TECHNOLOGY |
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Address after: 541004 c413-5, 4th floor, block a, information incubation building, No. D-12, information industry park, Qixing District, Guilin City, Guangxi Zhuang Autonomous Region Patentee after: Guangxi Derun Environmental Protection Technology Co.,Ltd. Address before: 541004 c413-5, 4th floor, block a, information incubation building, No. D-12, information industry park, Qixing District, Guilin City, Guangxi Zhuang Autonomous Region Patentee before: Guilin Derun Testing Co., Ltd |